홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Pyridine → HCID 22013556, 화합물

HRID 1532578
노트
인쇄 미리보기

반응식

HRID 1532578 반응식
[F:1][C:2]1[C:3]([C:9]2[C:13]([CH3:14])=[C:12]([C:15](=O)[NH2:16])[N:11]([CH3:18])[N:10]=2)=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.N1C=CC=CC=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O>O1CCOCC1>[F:1][C:2]1[C:3]([C:9]2[C:13]([CH3:14])=[C:12]([C:15]#[N:16])[N:11]([CH3:18])[N:10]=2)=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 9845Trifluoroacetic anhydrideHCID 22013571HCID 22013571, 화합물

생성물 1

HCID 22013556HCID 22013556, 화합물수율 94.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
22 °C

실험 절차

1.82 g of 3-(3-fluoro-5-chloro-2-pyridyl)-4-methyl-5-carbamoyl-1-methyl-[1H]-pyrazole (Example H44) are suspended in 20 ml of dioxane. First 1.65 ml of pyridine and then 1.44 ml of trifluoroacetic anhydride are added, while cooling in an ice-bath. 5 minutes later, the cooling bath is removed and the mixture is stirred at 22° C. for 1 hour. The brown-red solution is diluted with diethyl ether and washed with one molar hydrochloric acid and then with brine. After drying over sodium sulfate and filtering, the filtrate is concentrated directly together with twice the amount of silica gel. After application of this silica gel to a flash column, the column is eluted with n-hexane/ethyl acetate 4/1. 1.60 g of the desired title compound are obtained as a beige solid of melting point 144-146° C.

후처리

  1. temperaturewhile cooling in an ice-bath
  2. custom5 minutes later, the cooling bath is removed
  3. additionThe brown-red solution is diluted with diethyl ether
  4. washwashed with one molar hydrochloric acid
  5. dry with materialAfter drying over sodium sulfate
  6. filtrationfiltering
  7. concentrationthe filtrate is concentrated directly together with twice the amount of silica gel
  8. washAfter application of this silica gel to a flash column, the column is eluted with n-hexane/ethyl acetate 4/1

출처 및 근거

ORD 기록
ord-2d4e2065f1424bb7a6c859231425c784
출처 데이터셋
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06204221B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트